TWI856891B - Antistatic, anti-pilling, antibacterial and warm-keeping functional fiber and preparation method thereof - Google Patents

Abstract

An anti-static, anti-pilling, anti-bacterial and warm-keeping functional fiber and a preparation method thereof. The anti-static, anti-pilling, anti-bacterial and warm-keeping functional fiber comprises steps (a) to (c) described in the specification, and the anti-static, anti-pilling, anti-bacterial and warm-keeping functional fiber comprising a nitrile fiber body and a plurality of porous spheres is prepared. Because of the plant-derived powder in step (a), the anti-static, anti-pilling, antibacterial and thermal insulation functional fiber has good anti-static and antibacterial properties; combined with the pre-driver in step (a), the anti-static, anti-pilling, antibacterial and thermal insulation functional fiber also has good thermal insulation properties; combined with the radiation treatment in step (c), the anti-static, anti-pilling, antibacterial and thermal insulation functional fiber also has good anti-pilling properties; in addition, the average particle size of the plant-derived powder in step (a) is limited to 200 to 500 nm and the mass proportion of the porous spheres in step (b) is limited to 2 to 10wt%, so that step (c) can be carried out smoothly.

Description

Antistatic, anti-pilling, antibacterial and warm-keeping functional fiber and preparation method thereof

The present invention relates to a fiber and a preparation method thereof, and in particular to a multifunctional fiber and a preparation method thereof.

Acrylic is a synthetic fiber composed of acrylonitrile copolymers with an acrylonitrile content of more than 85% (mass percentage). Acrylic is also called "synthetic wool" because its properties are very similar to natural wool. It is not only fluffy, curly and soft, but also 15% warmer than natural wool. It is now widely used in clothing, home textiles, baby products, etc., and is mostly used in autumn and winter products.

When worn by users, clothing made of nitrile has at least the following three disadvantages: (1) Friction between fibers easily causes charge accumulation, thus generating static electricity; (2) Nitrile has good anti-bending properties, so even if the fibers rub against each other, they are not likely to fall off, but will easily cause fuzzing, pilling, and even the generation of microplastics, which has an adverse effect on the aesthetics of the clothing and the ecological environment; and (3) Since nitrile itself has a compact structure and does not have good breathability, sweat easily accumulates and breeds bacteria, which has an adverse effect on the user's skin health.

In addition, with the upgrading of consumption concepts, people have higher requirements for the functions of textiles. For example, the demand for textiles in autumn and winter not only needs to keep out the cold and keep warm, but also needs to effectively prevent the spread of pathogenic microorganisms. However, the current technology can only make nitrile have a single function of anti-static or anti-pilling or anti-bacterial or warm-keeping, but cannot make nitrile have multiple functions at the same time.

For example, Chinese Patent Publication No. 101818386 discloses a method for preparing anti-pilling nitrile fiber, which comprises mixing 93.5-94.5wt% acrylonitrile, 5.25-6.05wt% vinyl acetate and 0.25-0.45wt% sodium methyl propylene sulfonate, adjusting the concentration of the mixed monomers to 30-40wt%, and continuously carrying out aqueous phase suspension polymerization at 58-62°C and pH 2.5-3.5; the polymer after the reaction is terminated by chelation reaction, unreacted monomers are removed by a stripping tower, and then the polymer is washed with a filter to remove salt and water, and then granulated and formed by filtration. The powdered polymer obtained by drying is mixed and dissolved with dimethylacetamide, and the obtained spinning solution is heated, cooled, filtered, and then spun at a pressure of 0.7-0.9 MPa and a temperature of 90-95°C after temperature and pressure adjustment and filtering. The concentration of dimethylacetamide coagulation bath is 40-50wt%, and the coagulation bath temperature is 38-50°C. After double diffusion molding, washing, oiling, drying, and curling, the stretching multiple is 4-7 times, and the anti-pilling nitrile fiber is obtained by shaping at a shaping pressure of 120-200KPa, and the anti-pilling performance level is greater than level 4 and the hook strength is 0.6±0.2CN/dtex. The anti-pilling nitrile fiber produced by the Chinese patent publication has only the single function of anti-pilling.

Therefore, in order to make nitrile fiber have multifunctionality, one object of the present invention is to provide a novel anti-static, anti-pilling, anti-bacterial and warm-keeping functional fiber.

Therefore, the anti-static, anti-pilling, anti-bacterial and warm-keeping functional fiber of the present invention comprises a nitrile fiber body and a plurality of porous spheres embedded in the nitrile fiber body. Each porous sphere comprises a plant-derived core layer and a porous shell layer covering the plant-derived core layer. The porous spheres are prepared by drying a gel, which is formed by subjecting a first mixture comprising a plant-derived powder, an alkaline solution and a component solution including a precursor to a sol-gel reaction. The plant-derived core layer is composed of the plant-derived powder, which is selected from at least one of paclitaxel, clove extract, artemisia annua extract, chlorogenic acid, grape extract, sweet orange extract, dandelion extract, protein powder and water-soluble ginger extract, and the average particle size of the plant-derived powder ranges from 200nm to 500nm. The precursor is selected from at least one of nanocellulose, collagen, soy protein, phenolic resin-hexamethylenetetramine and ethyl silicate.

Another object of the present invention is to provide a novel method for preparing anti-static, anti-pilling, anti-bacterial and warm-keeping functional fiber.

Therefore, the preparation method of the anti-static, anti-pilling, antibacterial and warm-keeping functional fiber of the present invention comprises the following steps: (a). A first mixture comprising a plant-based powder, an alkaline solution and a component solution including a precursor is subjected to a sol-gel reaction to form a gel, and the gel is dried to obtain a plurality of porous spheres. The porous sphere comprises a plant-based core layer and a porous shell layer covering the plant-based core layer. The plant-based core layer is composed of the plant-based powder, and the plant-based powder is selected from at least one of paclitaxel, clove extract, artemisia annua extract, chlorogenic acid, grape extract, sweet orange extract, dandelion extract, protein powder and water-soluble ginger extract, and the average particle size of the plant-based powder ranges from 200nm to 500nm. The precursor is selected from at least one of nanocellulose, collagen, soy protein, phenolic resin-hexamethylenetetramine and ethyl silicate. (b) The second mixture comprising acrylonitrile, vinyl acetate and the porous spheres is polymerized to form a spinning stock solution, wherein the mass proportion of the porous spheres ranges from 2wt% to 10wt% based on the total amount of the spinning stock solution as 100wt%. (c). The spinning stock solution is spun to form primary fibers, and the primary fibers are sequentially irradiated and processed to obtain anti-static, anti-pilling, antibacterial and warm-keeping functional fibers, wherein the irradiation treatment is selected from at least one of electron beam irradiation, cobalt-60 irradiation and gamma ray irradiation.

The efficacy of the present invention is that in the anti-static, anti-pilling, antibacterial and warm-keeping functional fiber of the present invention, because each porous sphere includes the plant-based core layer with anti-static, anti-pilling and antibacterial functions, and the porous shell layer with warm-keeping function and covering the plant-based core layer, the anti-static, anti-pilling, antibacterial and warm-keeping functional fiber is jointly endowed with good anti-static, anti-pilling, antibacterial and warm-keeping functions. The preparation method of the anti-static, anti-pilling, antibacterial and warm-keeping functional fiber of the present invention comprises the following steps: adding the plant-based powder in step (a) so that the prepared anti-static, anti-pilling, antibacterial and warm-keeping functional fiber has anti-static and antibacterial functions; adding the precursor in step (a) so that the anti-static, anti-pilling, antibacterial and warm-keeping functional fiber also has a warm-keeping function; and combining the plant-based powder with the specific type of radiation treatment in step (c) so that the anti-static, anti-pilling, antibacterial and warm-keeping functional fiber also has an anti-pilling function and can be used as a nitrile fiber. In addition, since each porous sphere in step (a) includes the plant-derived core layer with anti-static, anti-pilling and antibacterial functions, and the porous shell layer with warm-keeping function and covering the plant-derived core layer, the anti-static, anti-pilling, antibacterial and warm-keeping functional fiber is endowed with good anti-static, anti-pilling, antibacterial and warm-keeping functions. Furthermore, the average particle size range of the plant-derived powder in step (a) is limited to 200nm to 500nm and the mass ratio range of the porous spheres in step (b) is limited to 2wt% to 10wt%, so that the spinning process in step (c) can be carried out smoothly.

The present invention is described in detail below.

〈Anti-static, anti-pilling, anti-bacterial and warm functional fiber〉

The anti-static, anti-pilling, anti-bacterial and warm-keeping functional fiber of the present invention comprises a nitrile fiber body and a plurality of porous spheres embedded in the nitrile fiber body.

The constituent material of the nitrile fiber body is acrylonitrile-vinyl acetate copolymer, and the acrylonitrile-vinyl acetate copolymer contains acrylonitrile in an amount of 85% (mass percentage) or more.

Each porous sphere includes a plant-derived core layer and a porous shell layer covering the plant-derived core layer. Each porous sphere is in the shape of an ellipse or a perfect sphere.

The porous spheres are prepared by drying a gel formed by subjecting a first mixture comprising a plant source powder, an alkaline solution and a component solution including a precursor to a sol-gel reaction.

The plant-derived core layer is composed of the plant-derived powder, which is selected from at least one of paclitaxel, clove extract, artemisia annua extract, chlorogenic acid, grape extract, sweet orange extract, dandelion extract, protein powder and water-soluble ginger extract, and the average particle size of the plant-derived powder ranges from 200nm to 500nm. The plant-derived core layer composed of the plant-derived powder allows the anti-static, anti-pilling, antibacterial and warm-keeping functional fiber to not only have good anti-static, anti-pilling and antibacterial functions, but also has colorability, moisture absorption and fluffiness. Because the particle size of the plant-derived powder ranges from 200nm to 500nm, the average particle size of the porous spheres ranges from 1μm or less, thereby ensuring that subsequent spinning can proceed smoothly and continuously. In addition, the average particle size of the porous spheres is below 1 μm, which meets the industry requirement that the average particle size of additive particles in the spinning process must be less than 2 μm.

The precursor is selected from at least one of nanocellulose, collagen, soy protein, phenolic resin-hexamethylenetetramine and ethyl silicate. The porous shell layer formed by the precursor allows the anti-static, anti-pilling, antibacterial and warm-keeping functional fiber to have not only a warm-keeping function but also a high degree of fluffiness. In addition, because the porous shell layer formed by the precursor is a porous mesh structure, the porous shell layer can also absorb odorous gases by physical adsorption to achieve a deodorizing effect.

In some embodiments of the present invention, based on 100 wt% of the total amount of each porous sphere, the mass proportion of the plant-based core layer ranges from 20 wt% to 30 wt%.

〈Preparation method of anti-static, anti-pilling, anti-bacterial and warm-keeping functional fiber〉

The preparation method of the anti-static, anti-pilling, antibacterial and warm-keeping functional fiber of the present invention comprises the following steps: (a). A first mixture comprising plant-based powder, alkaline solution and component solution is subjected to a sol-gel reaction to form a gel, and the gel is dried to obtain a plurality of porous spheres. (b). A second mixture comprising acrylonitrile, vinyl acetate and the porous spheres is subjected to a polymerization reaction to form a spinning stock solution. (c). The spinning stock solution is subjected to a spinning treatment to form a primary fiber, and the primary fiber is subjected to a radiation treatment and a processing treatment in sequence to obtain an anti-static, anti-pilling, antibacterial and warm-keeping functional fiber.

In the step (a), each porous sphere includes a plant-based core layer and a porous shell layer covering the plant-based core layer, wherein the plant-based core layer is composed of the plant-based powder.

If the average particle size of the plant-derived powder is less than 200 nm, the plant-derived powder is easy to agglomerate and settle in the first mixture. If the average particle size of the plant-derived powder is greater than 500 nm, the reaction time of the sol-gel reaction will be prolonged, and the spinning process of the step (c) will not proceed smoothly. Therefore, in the present invention, the average particle size of the plant-derived powder ranges from 200 nm to 500 nm. Furthermore, because the average particle size of the plant-derived powder ranges from 200 nm to 500 nm, the average particle size of the porous spheres ranges from 1 μm or less, thereby ensuring that the spinning process of the step (c) can proceed smoothly.

In some embodiments of the present invention, the plant-derived powder is selected from at least one of paclitaxel, clove extract, artemisia annua extract, chlorogenic acid, grape extract, sweet orange extract, dandelion extract, protein powder and water-soluble ginger extract, so that the anti-static anti-pilling antibacterial warm-keeping functional fiber not only has anti-static anti-pilling and antibacterial functions, but also has colorability, moisture absorption and fluffiness. In particular, by matching the plant-derived powder with the specific type of the radiation treatment in step (c), the anti-static anti-pilling antibacterial warm-keeping functional fiber also has anti-pilling function and is applied as nitrile fiber.

The component solution includes a precursor and a solvent. In some embodiments of the present invention, the precursor is selected from at least one of nanocellulose, collagen, soy protein, phenolic resin-hexamethylenetetramine and ethyl silicate, so that the anti-static anti-pilling antibacterial warm-keeping functional fiber not only has a warm-keeping function but also has a high degree of fluffiness. In addition, because the porous shell layer formed by the precursor is a porous mesh structure, the porous shell layer can also absorb odorous gases by physical adsorption to play a deodorizing role. It is worth mentioning that if the plant-based powder and the precursor are directly used for spinning, the plant-based powder and the precursor are easily lost during the spinning process, so that the formed fiber cannot actually have sufficient anti-static, anti-pilling, antibacterial and warm-keeping functions; on the contrary, in the present invention, because the porous shell layer covers the plant-based core layer, the anti-static, anti-pilling, antibacterial and warm-keeping functional fiber produced has sufficient porous spheres even after a complex spinning process and does have good anti-static, anti-pilling, antibacterial and warm-keeping functions, and even the anti-static, anti-pilling, antibacterial and warm-keeping functional fiber still retains good anti-static, anti-pilling and antibacterial functions after multiple washings. The type of the solvent is not limited, as long as it can dissolve the precursor and does not adversely affect the sol-gel reaction, it is suitable as the solvent. Specifically, in some embodiments of the present invention, the solvent is selected from at least one of dimethyl sulfoxide, N,N-dimethylformamide, formaldehyde and water.

The alkaline solution includes a solute and a solvent. The type of the solute and the concentration of the alkaline solution are not limited, as long as the compound that makes the alkaline solution alkaline and can undergo the sol-gel reaction with the plant-derived powder and the component solution is suitable as the solute. In some embodiments of the present invention, the solute is selected from at least one of sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate and ammonia monohydrate (NH ₃ ·H ₂ O). In some embodiments of the present invention, the concentration of the alkaline solution is 1wt% to 15wt%. The type of the solvent is not limited, as long as the liquid that can dissolve the precursor is suitable as the solvent. In some embodiments of the present invention, the solvent is selected from at least one of water and ethanol.

The structure and function of the porous spheres are as described above and will not be described in detail here. In order to make the porous spheres have a spherical shape of uniform size and be uniformly dispersed in the spinning stock solution of the step (b), in some embodiments of the present invention, the plant source powder and the alkaline solution are first mixed to form a mixed solution, and then the component solution is added dropwise to the mixed solution to form the first mixture. The dropwise addition speed ranges from 1 d/s to 2 d/s, the rotation speed ranges from 1500 r/min to 2000 r/min, the sol-gel reaction time ranges from 30 min to 60 min, the drying pressure ranges from -0.1 MPa to -0.02 MPa, the drying temperature ranges from -50°C to -10°C, and the drying time ranges from 6 hr to 12 hr.

In some embodiments of the present invention, the mass ratio of the plant source powder to the precursor in the first mixture ranges from 1:2 to 5.

In some embodiments of the present invention, based on 100 wt% of the total amount of each porous sphere, the mass proportion of the plant-based core layer ranges from 20 wt% to 30 wt%.

In the step (b), if the mass proportion of the porous spheres is less than 2wt% with the total amount of the spinning stock solution being 100wt%, the anti-static, anti-pilling, antibacterial and thermal insulation functional fiber obtained cannot have both antibacterial and thermal insulation functions, or one of the antibacterial and thermal insulation functions does not meet the industry requirements. If the mass proportion of the porous spheres is greater than 10wt%, the spinning process of the step (c) cannot be carried out smoothly. Therefore, in the present invention, the mass proportion of the porous spheres is in the range of 2wt% to 10wt% with the total amount of the spinning stock solution being 100wt%.

In some embodiments of the present invention, the mass ratio of the acrylonitrile, the vinyl acetate and the porous spheres is in the range of 8-10:0.8-1.1:2-10.

In some embodiments of the present invention, the second mixture further comprises an initiator and a reaction solution for promoting the polymerization reaction. In some embodiments of the present invention, the initiator is selected from azobisisobutyronitrile, and the mass ratio of the initiator is in the range of 0.80wt% to 1.15wt% based on the total amount of the acrylonitrile as 100wt%. In some embodiments of the present invention, the reaction solution is selected from a sodium thiocyanate aqueous solution with a concentration range of 40wt% to 50wt%.

In step (c), the radiation treatment is selected from at least one of electron beam irradiation, cobalt-60 irradiation and gamma ray irradiation. By subjecting the nascent fiber to the radiation treatment, not only can the rigidity of the nascent fiber be weakened, thereby making the anti-pilling grade of the anti-static anti-pilling antibacterial warm-keeping functional fiber meet international requirements, but also the washing resistance, coloring rate and moisture absorption of the anti-static anti-pilling antibacterial warm-keeping functional fiber can be improved.

In some embodiments of the present invention, the spinning process includes stirring, filtering, defoaming, heating and spinning in sequence. Specifically, the spinning stock solution is stirred, filtered and defoamed in sequence under nitrogen protection to obtain a pre-treated spinning solution, and then the pre-treated spinning solution is heated and spinning is performed to obtain the spun fiber.

In some embodiments of the present invention, the processing includes washing, stretching, oiling, drying and shaping in sequence.

The meanings of the spinning process and the processing process include the meanings commonly understood and used by people familiar with the textile technology field, and the specific operating steps and conditions are well known to people familiar with the textile technology field and can be flexibly adjusted according to needs, so they will not be elaborated here.

In some embodiments of the present invention, the heating temperature ranges from 80°C to 90°C.

In some embodiments of the present invention, the temperature range of the radiation treatment is 10°C to 40°C, and the time of the radiation treatment is 30 sec to 120 sec.

In some embodiments of the present invention, the water washing temperature ranges from 60°C to 90°C, and the water washing flow rate ranges from 2500 L/h to 3500 L/h.

In some embodiments of the present invention, the stretching multiple ranges from 3.5 times to 6.0 times, and the speed ranges from 30 m/min to 60 m/min.

In some embodiments of the present invention, the dry breaking strength of the anti-static anti-pilling antibacterial warm-keeping functional fiber ranges from 3.0 cN/dtex or more. In some embodiments of the present invention, the dyeing rate of the anti-static anti-pilling antibacterial warm-keeping functional fiber ranges from 80% to 90%. In some embodiments of the present invention, the moisture regain of the anti-static anti-pilling antibacterial warm-keeping functional fiber ranges from 5% to 8%. In some embodiments of the present invention, the fluffiness of the anti-static anti-pilling antibacterial warm-keeping functional fiber ranges from 20 cm ³ /g to 25 cm ³ /g. In some embodiments of the present invention, the anti-pilling grade of the anti-static anti-pilling antibacterial warm-keeping functional fiber ranges from grade 4 to grade 5. In some embodiments of the present invention, the fiber fineness of the anti-static anti-pilling antibacterial warm-keeping functional fiber ranges from 0.5 dtex to 2.0 dtex. In order to make the anti-static anti-pilling antibacterial warm-keeping functional fiber also have soft, thin and breathable properties, preferably, the fiber fineness of the anti-static anti-pilling antibacterial warm-keeping functional fiber ranges from 0.5 dtex to 1.0 dtex.

The present invention will be further described with respect to the following embodiments, but it should be understood that the embodiments are only for illustration and description and should not be construed as limitations on the implementation of the present invention.

〈Implementation Example 1 〉

(a). Add plant-derived powder (type is paclitaxel; average particle size is 200nm) to an alkaline solution (solute is monohydrated ammonia; solvent is water) with a solute concentration of 10wt% and stir thoroughly to form a mixed solution in which the mass proportion of the plant-derived powder is 5wt%. Then, add the component solution (precursor is ethyl silicate, and the mass of the precursor is 3 times the mass of the plant-derived powder; solvent is water) dropwise to the mixed solution at a drip rate of 1d/s to obtain a first mixture. In the first mixture, the mass ratio of the plant-derived powder to the precursor is 1:3. Then, the first mixture is subjected to a sol-gel reaction at room temperature (25°C) at a rotation speed of 1800r/min for 50min and allowed to stand to obtain a gel. The gel was then dried for 10 hours at -0.05 MPa and -30°C to obtain a plurality of porous spheres with an average particle size of 0.6 μm. Each porous sphere includes a plant-derived core layer formed by the plant-derived powder and a porous shell layer formed by the precursor and covering the plant-derived core layer. The mass of the plant-derived core layer accounts for 27 wt% based on the total amount of each porous sphere being 100 wt%.

(b) Mix acrylonitrile, vinyl acetate, the porous spheres, an initiator (azobisisobutyronitrile) and a reaction solution (a sodium thiocyanate aqueous solution) with a concentration of 45 wt% to obtain a second mixture. In the second mixture, the mass ratio of acrylonitrile, vinyl acetate and the porous spheres is 9:1:7, and the total proportion of acrylonitrile, vinyl acetate and the porous spheres is greater than 85%, and the mass ratio of the initiator to the acrylonitrile is 1:100. Then, the second mixture is polymerized at 55°C for 50 minutes to obtain a spinning stock solution.

(c) The spinning stock solution is spun to form spun fibers. The detailed process is that the spinning stock solution is stirred, filtered and defoamed in sequence under nitrogen protection to obtain a pre-treated spinning solution, and then the pre-treated spinning solution is heated at 85°C and extruded from a spray plate to form the spun fibers. The spun fibers are then irradiated and processed in sequence to obtain anti-static, anti-pilling, anti-bacterial and warm-keeping functional fibers. The operating parameters of the radiation treatment are as follows: the specific type is electron beam radiation, the radiation dose is 53 kGy, the temperature is 25°C, and the time is 90 seconds. The processing includes washing, stretching, oiling, drying and shaping in sequence. The operating parameters of the washing are as follows: temperature is 80°C, flow rate is 3000L/h. The operating parameters of the stretching are as follows: stretching multiple is 4.5 times, speed is 50m/min.

〈Implementation Example 2 and 3 〉

Examples 2 and 3 are carried out with similar steps to Example 1, except that the parameter conditions of each step are changed, as shown in Table 1.

〈Comparison Example 1 to 5 〉

The differences between Comparative Examples 1 to 5 and Example 1 are: Comparative Example 1 does not perform step (a), and in step (b), the porous spheres are replaced by "precursor"; Comparative Example 2 does not perform step (a), and in step (b), the porous spheres are replaced by "plant source powder"; Comparative Example 3 does not perform the irradiation of step (c); Comparative Examples 4 and 5 change the type of radiation, as shown in Table 1.

〈Evaluation Items〉

The anti-static, anti-pilling, anti-bacterial and warm-keeping functional fibers of Examples 1 to 3 and Comparative Examples 1 to 5 were tested for the following evaluation items, and the test results are shown in Table 2.

Anti-static test: refer to the standard test method GB/T 14342-2015 "Chemical fiber staple fiber specific resistance test method".

Anti-pilling test: refer to the standard test method GB/T 4802.2-2008 "Textiles - Determination of pilling properties of fabrics - Part 2: Modified Martindale method".

Antibacterial test: Refer to the standard test method GB/T 20944.3-2008 "Evaluation of antibacterial properties of textiles Part 3: Oscillation method". The strains used in the antibacterial test are the following four types: Staphylococcus aureus, Escherichia coli, Klebsiella pneumoniae and Moraxella.

Washing test: refer to the standard test method GB/T 3921-2008 "Textiles-Color fastness test-Color fastness to washing with soap".

Warmth test: Refer to the standard test method GB/T 30127-2013 "Textiles - Testing and evaluation of far-infrared performance".

Property test-dry breaking strength: refer to the standard test method GB/T 14337-2022 "Chemical fibers-Test method for tensile properties of staple fibers".

Property test – Dyeing rate: refer to the standard test method GB/T 16602-2008 "Acrylic staple fibers and tow" Appendix A.

Property test – Moisture regain: refer to the standard test method GB/T 9995-1997 "Determination of moisture content and moisture regain of textile materials - Oven drying method".

Property test – Fluff: Refer to the standard test method SN/T 4237-2015 “Test method for the fluff of down for import and export – Multifunctional fluff meter test method”.

Purity test – whiteness: refer to the standard test method GB/T 17644-2008 “Test method for whiteness and color of textile fibers”.

Purity test – Acrylonitrile content: Refer to standard test method FZ-T 01057-2007 "Test method for identification of textile fibers".

Table 1 Preparation method Embodiment Comparison Example 1 2 3 1 2 3 4 5 (a) Preparation of porous spheres Plant source powder Type Paclitaxel Clove extract and paclitaxel in a 1:1 mass ratio Dandelion extract and paclitaxel in a 1:1 mass ratio without without Paclitaxel Paclitaxel Paclitaxel Average particle size (nm) 200 500 400 200 200 200 Alkaline solution Solute type Ammonia Monohydrate Ammonia Monohydrate Ammonia Monohydrate Ammonia Monohydrate Ammonia Monohydrate Ammonia Monohydrate Solvent type water water water water water water Concentration(wt%) 10 1 15 10 10 10 Component solution Propellant type Ethyl silicate Ethyl silicate Ethyl silicate Ethyl silicate Ethyl silicate Ethyl silicate Solvent type water water water water water water Dripping rate (d/s) 1 2 1 1 1 1 Mass ratio of plant-derived powder to precursor 1:3 1:2 1:5 1:3 1:3 1:3 Sol-gel reaction Speed (r/min) 1800 2000 2000 1800 1800 1800 Time(min) 50 30 60 50 50 50 Dry Pressure(MPa) -0.05 -0.10 -0.02 -0.05 -0.05 -0.05 Temperature(℃) -30 -50 -10 -30 -30 -30 Time(hr) 10 6 12 10 10 10 Porous sphere Average particle size (μm) 0.6 1.0 0.8 0.6 0.6 0.6 Mass ratio of plant-derived powder (wt%) 27 20 30 27 27 27 (b) Preparation of spinning stock solution Mass ratio of acrylonitrile, vinyl acetate and porous spheres 9:1:7 8:0.8:2 10:1.1:10 The difference from Example 1 is that the porous spheres are replaced with "ethyl silicate" The difference from Example 1 is that the porous spheres are replaced with "paclitaxel" 9:1:7 9:1:7 9:1:7 Mass ratio of initiator to acrylonitrile 1:100 0.80:100 1.15:100 1:100 1:100 1:100 Reaction solution Concentration(wt%) 45 40 50 45 45 45 Polymerization Temperature(℃) 55 45 60 55 55 55 Time(min) 50 50 60 50 50 50 (c). Preparation of anti-static, anti-pilling, anti-bacterial and warm functional fibers Heating Temperature(℃) 85 80 90 85 85 85 85 85 Radiation treatment Type Electron beam irradiation without Ultraviolet radiation Microwave radiation Radiation dose (kGy) 53 twenty one 60 53 53 53 53 Temperature(℃) 25 10 40 25 25 25 25 Time(sec) 90 120 120 90 90 90 90 Washing Temperature(℃) 80 60 90 80 80 80 80 80 Flow rate (L/h) 3000 2500 3500 3000 3000 3000 3000 3000 Stretch Extension multiple (times) 4.5 3.5 6.0 4.5 4.5 4.5 4.5 4.5 Speed(m/min) 50 30 60 50 50 50 50 50

Table 2 Evaluation items Embodiment Comparison Example 1 2 3 1 2 3 4 5 Anti-static test Resistivity(Ω·cm) 5.8×10 ⁵ 6.2×10 ⁵ 5.0×10 ⁵ 1.0×10 ⁶ 1.5×10 ⁷ -- -- -- Anti-pilling test Anti-pilling grade(grade) 5 4 5 -- -- 2 -- -- Antibacterial test Average antibacterial rate (%) 98.2 96.8 99.1 52.0 ^* 75.0 -- -- -- Washability test Average antibacterial rate after 100 washes (%) 96.5 94.0 96.9 -- ^# 43.0 73.5 -- -- Warmth test Far infrared emissivity 0.90 0.88 0.93 0.85 0 -- -- -- Maximum temperature difference before and after far infrared heating (℃) 14 12 15 10 0 -- -- -- Property test Dry breaking strength (cN/dtex) 3.73 3.36 3.45 3.10 2.75 3.12 -- -- Coloring rate (%) 86 80 90 -- -- 55 -- -- Moisture regain (%) 6 5 8 -- -- 2 -- -- Fluff (cm ³ /g) 25 20 twenty three -- -- 18 -- -- Purity test Whiteness(%) 85 83 84 -- -- -- 80 75 Acrylonitrile content (%) ≥ 87 ≥ 87 ≥ 87 -- -- -- 84 83 Notes: 1. "--" indicates that the test was not conducted. 2. "*" indicates that Moraxella cannot be killed. 3. "#" indicates that the water washing test was not conducted because the average inhibition rate was too low. 4. The average inhibition rate is the average result of three tests on a single strain (Staphylococcus aureus).

As shown in Table 2, the anti-static, anti-pilling, antibacterial and thermal insulation functional fibers of Examples 1 to 3 have good anti-static, good anti-pilling, good antibacterial, good water washability, good thermal insulation, good tensile strength, good dyeing rate, good moisture absorption (moisture regain), good bulkiness, good whiteness and an acrylonitrile content of more than 85%.

Furthermore, compared with Comparative Example 2 in which paclitaxel is used to prepare the spinning stock solution, the anti-static, anti-pilling, antibacterial and warm-keeping functional fibers of Examples 1 to 3 in which porous spheres are used to prepare the spinning stock solution have better anti-static, antibacterial, water-washing and warm-keeping functions, which verifies that the structural design of the porous shell layer in the porous spheres covering the plant-based core layer still allows the prepared anti-static, anti-pilling, antibacterial and warm-keeping functional fibers to have good anti-static, antibacterial and warm-keeping functions even after the multiple procedures in step (c), and also allows the prepared anti-static, anti-pilling, antibacterial and warm-keeping functional fibers to have good water-washing resistance even after multiple washing tests.

Compared with the comparative example 3 which is not irradiated, the anti-static anti-pilling antibacterial warm-keeping functional fibers of the irradiated examples 1 to 3 have better anti-pilling function. In addition, compared with the comparative example 4 which uses ultraviolet radiation and the comparative example 5 which uses microwave radiation, the anti-static anti-pilling antibacterial warm-keeping functional fibers of the electron beam irradiated examples 1 to 3 have better acrylonitrile content (more than 85%) and can be used as nitrile fibers.

However, the above is only an embodiment of the present invention and should not be used to limit the scope of implementation of the present invention. All simple equivalent changes and modifications made according to the scope of the patent application of the present invention and the content of the patent specification are still within the scope of the present invention.

Claims (9)

A method for preparing an anti-static, anti-pilling, antibacterial and warm-keeping functional fiber comprises the following steps: (a) subjecting a first mixture comprising a plant-based powder, an alkaline solution and a component solution comprising a precursor to a sol-gel reaction to form a gel, and drying the gel to obtain a plurality of porous spheres, wherein each porous sphere comprises a plant-based core layer and a porous shell layer covering the plant-based core layer, the plant-based core layer being composed of the plant-based powder, the plant-based powder being selected from at least one of paclitaxel, clove extract, artemisia annua extract, chlorogenic acid, grape extract, sweet orange extract, dandelion extract, protein powder and water-soluble ginger extract, and the average particle size of the plant-based powder is in the range of 200 nm to 500 nm. nm, the precursor is selected from at least one of nanocellulose, collagen, soy protein, phenolic resin-hexamethylenetetramine and ethyl silicate; (b) polymerizing a second mixture comprising acrylonitrile, vinyl acetate and the porous spheres to form a spinning stock solution, wherein, based on the total amount of the spinning stock solution being 100wt%, the porous spheres The mass ratio ranges from 2wt% to 10wt%; and (c). The spinning stock solution is spun to form primary fibers, and the primary fibers are sequentially irradiated and processed to obtain anti-static, anti-pilling, anti-bacterial and warm-keeping functional fibers, wherein the irradiation treatment is selected from at least one of electron beam irradiation, cobalt-60 irradiation and gamma ray irradiation. The preparation method of the anti-static, anti-pilling, anti-bacterial and warm-keeping functional fiber as described in claim 1, wherein in step (a), the component solution also includes a solvent, and the solvent is selected from at least one of dimethyl sulfoxide, N,N-dimethylformamide, formaldehyde and water. The preparation method of the anti-static, anti-pilling, antibacterial and warm-keeping functional fiber as described in claim 1, wherein in step (a), the alkaline solution comprises a solute and a solvent, the solute is selected from at least one of sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate and ammonia monohydrate, the concentration of the alkaline solution ranges from 1wt% to 15wt%, and the solvent is selected from at least one of water and ethanol. The method for preparing anti-static, anti-pilling, anti-bacterial and warm-keeping functional fibers as described in claim 1, wherein in step (a), the mass ratio of the plant source powder to the precursor in the first mixture ranges from 1:2 to 5. The method for preparing anti-static, anti-pilling, anti-bacterial and warm-keeping functional fibers as described in claim 1, wherein in step (a), the mass proportion of the plant-based core layer ranges from 20wt% to 30wt%, based on the total mass of each porous sphere being 100wt%. The preparation method of the anti-static, anti-pilling, antibacterial and warm-keeping functional fiber as described in claim 1, wherein in the step (a), the plant source powder and the alkaline solution are first mixed to form a mixed solution, and then the component solution is added dropwise to the mixed solution to form the first mixture, the dropwise addition speed ranges from 1d/s to 2d/s, the rotation speed range of the sol-gel reaction ranges from 1500r/min to 2000r/min, the time range of the sol-gel reaction ranges from 30min to 60min, the drying pressure ranges from -0.1MPa to -0.02MPa, the drying temperature ranges from -50℃ to -10℃, and the drying time ranges from 6hr to 12hr. The method for preparing anti-static, anti-pilling, anti-bacterial and warm-keeping functional fibers as described in claim 1, wherein in step (b), the mass ratio of the acrylonitrile, the vinyl acetate and the porous spheres is in the range of 8 to 10: 0.8 to 1.1: 2 to 10. The method for preparing anti-static, anti-pilling, anti-bacterial and warm-keeping functional fibers as described in claim 1, wherein in step (c), the spinning process includes stirring, filtering, defoaming, heating and spinning in sequence, and the processing includes washing, stretching, oiling, drying and shaping in sequence. The method for preparing the anti-static, anti-pilling, anti-bacterial and warm-keeping functional fiber as described in claim 1, wherein in step (c), the temperature range of the radiation treatment is 10°C to 40°C, and the time of the radiation treatment is 30sec to 120sec.